Ultrafine denier polyester drawn textured yarn and its preparation method

Abstract

This invention relates to the field of fibers, and provides an ultrafine denier polyester textured yarn and its preparation method. By weight, the ultrafine denier polyester textured yarn comprises the following raw materials: 90-110 parts polyester, 0.6-2 parts functional filler, 1-4 parts lubricating dispersant, and 1-2 parts low-density polyethylene. The ultrafine denier polyester textured yarn provided by this invention is not easily broken during processing and also has good antibacterial properties.

Description

Technical Field

[0001] This invention relates to the field of fibers, and in particular to an ultrafine denier polyester stretch textured yarn and its preparation method. Background Technology

[0002] Polyester has the characteristics of high modulus, high strength, elasticity, good shape retention, and wrinkle resistance, making it an ideal textile material. It can be used to develop a variety of high-end fabrics and has a good market prospect. However, as people's living standards continue to improve, consumers' demands are also constantly increasing, and some of the shortcomings of polyester are becoming more and more obvious, such as poor moisture absorption and breathability, and a hand feel that is not as soft as cotton.

[0003] Microfiber is finer than conventional fibers. Compared to conventional fibers, microfiber polyester has a softer feel, better thermal insulation, and better moisture absorption and breathability. It effectively overcomes the shortcomings of natural fibers, such as wrinkling, and synthetic fibers, such as poor breathability. It is widely used in clothing, furniture fabrics, and other specialty fabrics. However, due to the extremely fine total fineness of microfiber polyester, it is prone to yarn breakage during production, which poses a challenge to the efficient production of microfiber polyester. Furthermore, improving the antibacterial properties of polyester fabrics is also crucial.

[0004] CN 108796654 A discloses a preparation process for high-strength ultrafine denier polyester fiber. It uses polyester chips with a viscosity of 0.68 as raw material, spins the fibers into fiber bundles through melt spinning, and then processes them through cooling, oiling, pre-networking, stretching and setting, main networking, and winding to achieve the desired finish. This process improves the product's softness, breathability, and moisture absorption, giving it a cotton-like feel. While the process improves the strength of the fibers to some extent, the 0.68 viscosity polyester chips used in this application have a relatively low molecular weight, short molecular chain length, and weak entanglement between molecular chains, resulting in inherently low fiber breaking strength. Furthermore, no fillers or other reinforcing materials are used, and no performance testing indicators are provided. It is unclear whether the fiber will break under repeated stretching.

[0005] Therefore, there is an urgent need in the market for an ultra-fine denier polyester stretch textured yarn that is not easily broken during processing and also has good antibacterial properties. Summary of the Invention

[0006] To address the problems existing in the prior art, this invention uses polyester as the matrix material, incorporates functional fillers, and synthesizes an ultra-fine denier polyester stretch textured yarn in combination with lubricating dispersants and low-density polyethylene. This solves the problems of easy breakage and poor antibacterial properties of ultra-fine denier polyester stretch textured yarn during processing.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: The present invention provides an ultrafine denier polyester stretch textured yarn, which, by weight, comprises the following raw materials: 90-110 parts polyester, 0.6-2 parts functional filler, 1-4 parts lubricant and dispersant, and 1-2 parts low-density polyethylene.

[0008] In some embodiments of the present invention, the polyester is spinning-grade polyethylene terephthalate chips.

[0009] In some embodiments of the present invention, the method for preparing the functional filler includes the following steps: (1) Add potassium hydroxide to an ethanol aqueous solution and stir to obtain a potassium hydroxide solution for later use. Add zinc acetate dihydrate to an ethanol aqueous solution and stir at 75-85℃ for 30-40 min. Cool to room temperature and add potassium hydroxide solution while stirring. Let it age for 30 min, centrifuge, wash, and then add to an ethanol aqueous solution to disperse. Add KH550, stir, centrifuge, wash the precipitate, freeze dry, and obtain zinc oxide particles for later use. (2) Add the modified polysiloxane to tetrahydrofuran, add the zinc oxide particles from step (1), stir, evaporate the solvent, and vacuum dry to obtain the functional filler.

[0010] In step (1), the mass ratio of zinc acetate dihydrate to potassium hydroxide and KH550 is 1:(0.4-0.6):(0.04-0.06).

[0011] In some embodiments of the present invention, in step (2), the mass ratio of zinc oxide particles to modified polysiloxane is 1:(1.5-2).

[0012] Preferably, in step (2), the mass ratio of zinc oxide particles to modified polysiloxane is 1:1.8.

[0013] In some embodiments of the present invention, step (2) of the preparation method of the modified polysiloxane includes the following steps: 1) Mix octamethylcyclotetrasiloxane and phenyltris(dimethylsiloxane)silane, add sulfuric acid aqueous solution, stir for 17-18 h, separate the sulfuric acid phase, add sodium bicarbonate, stir, filter, and distill the filtrate under reduced pressure to obtain product 1 for later use. 2) Add product 1 from step 1) into a reaction vessel, pass in an inert gas, add chloroplatinic acid-tetrahydrofuran solution, preheat tert-butyl methacrylate to 75-85℃ and add dropwise, add polymerization inhibitor, react for 8-10 hours, distill under reduced pressure, filter, collect the liquid, and obtain product 2 for later use. 3) Under an inert atmosphere, heat to 85-90℃, add concentrated sulfuric acid to product 2 from step 2), react for 2.5-3.5 hours, cool to room temperature, add to chloroform, wash, separate the chloroform phase, and rotary evaporate to obtain modified polysiloxane.

[0014] In some embodiments of the present invention, in step 1), the mass ratio of octamethylcyclotetrasiloxane to phenyltris(dimethylsiloxane)silane is 1:(0.15-0.4).

[0015] Preferably, in step 1), the mass ratio of octamethylcyclotetrasiloxane to phenyltris(dimethylsiloxane)silane is 1:0.25.

[0016] In some embodiments of the present invention, in step 2), the mass ratio of product 1 to tert-butyl methacrylate is 1:(0.4-0.55).

[0017] Preferably, in step 2), the mass ratio of product 1 to tert-butyl methacrylate is 1:0.5.

[0018] In some embodiments of the present invention, in step 3), the mass ratio of product 2 to concentrated sulfuric acid is 1:(0.008-0.015), wherein the concentration of concentrated sulfuric acid is 98wt%.

[0019] Preferably, in step 3), the mass ratio of product 2 to concentrated sulfuric acid is 1:0.01.

[0020] Ultrafine denier polyester has advantages such as a soft feel, good heat retention, and moisture absorption and breathability, but its yarn strength and antibacterial properties need to be improved. Nano zinc oxide has both good reinforcing effect and antibacterial properties, making it a good candidate for functional filler. However, nano zinc oxide alone has the problem of easy agglomeration and poor dispersibility.

[0021] The applicant first prepared zinc oxide by reacting potassium hydroxide with zinc acetate dihydrate, and then improved its dispersibility with silane coupling agent KH550 to obtain zinc oxide particles with uniform particle size and good dispersibility. Further, the applicant designed and synthesized a modified polysiloxane using octamethylcyclotetrasiloxane, phenyltris(dimethylsiloxane)silane, and tert-butyl methacrylate as raw materials, under the catalytic hydrolysis of concentrated sulfuric acid. This modified polysiloxane has a dendritic structure with multiple polysiloxane chain arms, each chain arm ending in a carboxyl group, which strengthens the hydrogen bonding between it and the polyester and provides better interfacial compatibility. Using the modified polysiloxane as the framework structure for composite zinc oxide particles, multiple carboxyl groups can simultaneously interact with the hydroxyl groups on the surface of the zinc oxide particles, effectively preventing particle agglomeration. In addition, the modified polysiloxane and zinc oxide particles can also form metal salt crosslinking, effectively enhancing the overall mechanical properties and stability of the functional filler.

[0022] In some embodiments of the present invention, the lubricating dispersant is polyethylene wax or oxidized polyethylene wax.

[0023] Preferably, the lubricating dispersant is oxidized polyethylene wax.

[0024] The applicant's addition of a certain amount of polyethylene wax or oxidized polyethylene wax as a lubricating dispersant can improve the smoothness and evenness of the yarn surface, making the yarn surface smoother, and at the same time reduce static electricity to a certain extent, further reducing the possibility of yarn breakage.

[0025] In some embodiments of the present invention, the density of the low-density polyethylene is 0.915-0.925 g / cm³. 3 .

[0026] In another aspect, the present invention provides a method for preparing the ultrafine denier polyester stretch textured yarn described in the above technical solution, comprising the following steps: After melting polyester, functional fillers, lubricating dispersants and low-density polyethylene are added, mixed and extruded to obtain yarn. After cooling, oiling, stretching, and texturing, ultra-fine denier polyester textured yarn is obtained.

[0027] Compared with the prior art, the present invention has the following beneficial effects: (1) This invention uses polyester as the main material, designs and adds functional fillers, and combines antistatic agents, flame retardants and antioxidants to synthesize an ultra-fine denier polyester stretch textured yarn. Through the synergistic effect between the components, the problems of easy breakage and poor antibacterial properties of ultra-fine denier polyester stretch textured yarn during processing are solved.

[0028] (2) In this invention, zinc oxide is first prepared by reacting potassium hydroxide with zinc acetate dihydrate, and then its dispersibility is improved by using silane coupling agent KH550 to obtain zinc oxide particles with uniform particle size and good dispersibility. Furthermore, the applicant designed and synthesized a modified polysiloxane, which was prepared by using octamethylcyclotetrasiloxane, phenyltris(dimethylsiloxane)silane and tert-butyl methacrylate as raw materials under the catalytic hydrolysis of concentrated sulfuric acid. The modified polysiloxane was used as the skeleton structure to composite zinc oxide particles, which improved the dispersibility of functional fillers, thereby enabling ultrafine denier polyester stretch textured yarn to have good breaking strength and antibacterial properties. Detailed Implementation

[0029] The present invention will be described below with reference to specific embodiments. It should be noted that the following embodiments are examples of the present invention and are used only to illustrate the invention, not to limit it. Other combinations and various modifications within the scope of the present invention can be made without departing from its spirit or scope.

[0030] In the following examples and comparative examples, except for the functional fillers, all other compound monomers and related reagents used were commercially available. The polyester was spinning-grade polyethylene terephthalate chips; the number-average molecular weight of the polyethylene wax and oxidized polyethylene wax was 2500; and the density of the low-density polyethylene was 0.92 g / cm³. 3 The model number for polydimethylsiloxane is MB50-011.

[0031] Preparation Example 1 The method for synthesizing modified polysiloxane-1 includes the following steps: 1) Mix 40g of octamethylcyclotetrasiloxane and 10g of phenyltris(dimethylsiloxane)silane, add 1.2g of 98wt% sulfuric acid aqueous solution, stir for 17.5h, separate the sulfuric acid phase, add 1.5g of sodium bicarbonate, stir for 30min and filter, distill the filtrate under reduced pressure (150℃, 1kPa, 3h) to obtain product 1 for later use; 2) Add 50g of product 1 from step 1) to a reaction vessel, purge with nitrogen, add 0.25ml of 0.1mol / L chloroplatinic acid-tetrahydrofuran solution, add 25g of tert-butyl methacrylate preheated to 80℃ and then add dropwise (1.5h), add 0.05g of p-hydroxyanisole, react for 9h, distill under reduced pressure at 120℃ and 1kPa for 2h, filter, collect the liquid, and obtain product 2 for later use; 3) Under a nitrogen atmosphere, heat to 85°C, add 0.4g of 98wt% concentrated sulfuric acid to 40g of product 2 from step 2), react for 3h, cool to room temperature, add to 50g of chloroform, wash with deionized water until pH=7, separate the chloroform phase, and rotary evaporate the solvent to obtain modified polysiloxane-1.

[0032] Preparation Example 2 Modified polysiloxane-2 is implemented in the same way as modified polysiloxane-1, except that the mass of phenyltris(dimethylsiloxane)silane in step 1) is replaced with 4g.

[0033] Preparation Example 3 Modified polysiloxane-3 is implemented in the same way as modified polysiloxane-1, except that the mass of tert-butyl methacrylate in step 2) is replaced with 17g.

[0034] Preparation Example 4 Modified polysiloxane-4 is implemented in the same way as modified polysiloxane-1, except that the mass of concentrated sulfuric acid in step 3) is replaced with 1g.

[0035] Preparation Example 5 The synthesis method of functional filler A includes the following steps: (1) Add 3.1g of potassium hydroxide to 50ml of 50wt% ethanol aqueous solution and stir for 30min to obtain potassium hydroxide solution for later use. Add 6g of zinc acetate dihydrate to 200ml of 50wt% ethanol aqueous solution and stir at 80℃ for 35min. Cool to room temperature and add potassium hydroxide solution while stirring. Let it age for 30min, centrifuge, wash, and then add to ethanol aqueous solution. Disperse evenly, add 0.3g of KH550, stir at 50℃ for 1h, centrifuge, wash the precipitate, and freeze dry at -50℃ for 24h to obtain zinc oxide particles for later use. (2) Add 9g of modified polysiloxane-1 to 30g of tetrahydrofuran, add 5g of zinc oxide particles from step (1), stir for 1.5h, evaporate the solvent, and vacuum dry at 60℃ for 12h to obtain functional filler A.

[0036] Preparation Example 6 Functional filler B is implemented in the same way as functional filler A, except that the mass of modified polysiloxane-1 in step (2) is replaced with 6g.

[0037] Preparation Example 7 Functional filler C is implemented in the same way as functional filler A, except that the mass of modified polysiloxane-1 in step (2) is replaced with 12g.

[0038] Preparation Example 8 Functional filler D is implemented in the same way as functional filler A, except that in step (2), modified polysiloxane-1 is replaced by modified polysiloxane-2 in equal amounts.

[0039] Preparation Example 9 Functional filler E is implemented in the same way as functional filler A, except that in step (2), modified polysiloxane-1 is replaced by modified polysiloxane-3 in equal amounts.

[0040] Preparation Example 10 Functional filler F is implemented in the same way as functional filler A, except that in step (2), modified polysiloxane-1 is replaced by modified polysiloxane-4 in equal amounts.

[0041] Preparation Example 11 Functional filler G is implemented in the same way as functional filler A, except that in step (2), the modified polysiloxane-1 is replaced by commercially available conventional polydimethylsiloxane.

[0042] Preparation Example 12 Functional filler H is implemented in the same way as functional filler A, except that functional filler A is replaced by zinc oxide particles obtained in step (1). Example 1

[0043] An ultrafine denier polyester textured yarn, by weight, comprises the following raw materials: 100 parts polyester, 1.5 parts functional filler A, 2.5 parts oxidized polyethylene wax, and 1.5 parts low-density polyethylene.

[0044] The preparation method of ultrafine denier polyester drawn textured yarn in this embodiment includes the following steps: After the polyester is melted, functional filler A, oxidized polyethylene wax and low-density polyethylene are added, mixed evenly, and extruded at 270°C to obtain yarn. After cooling, oiling, stretching (stretch ratio of 1.50DR), and texturing and shaping (setting temperature of 170°C) are performed to obtain ultra-fine denier polyester stretch textured yarn. Example 2

[0045] An ultrafine denier polyester textured yarn, by weight, comprises the following raw materials: 90 parts polyester, 0.6 parts functional filler A, 1 part oxidized polyethylene wax, and 1 part low-density polyethylene.

[0046] The preparation method of the ultrafine denier polyester stretch textured yarn in this embodiment is the same as in Embodiment 1. Example 3

[0047] An ultrafine denier polyester textured yarn, by weight, comprises the following raw materials: 110 parts polyester, 2 parts functional filler A, 4 parts polyethylene wax, and 2 parts low-density polyethylene.

[0048] The preparation method of ultrafine denier polyester drawn textured yarn in this embodiment includes the following steps: After the polyester is melted, functional filler A, polyethylene wax and low-density polyethylene are added, mixed evenly, and extruded at 270°C to obtain yarn. After cooling, oiling, stretching (stretch ratio of 1.50DR), and texturing and shaping (setting temperature of 170°C) are performed to obtain ultra-fine denier polyester stretch textured yarn. Example 4

[0049] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler B in an equal amount. Example 5

[0050] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler C in equal amounts. Example 6

[0051] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler D in equal amounts. Example 7

[0052] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler E in equal amounts. Example 8

[0053] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler F in equal amounts. Example 9

[0054] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler G in equal amounts. Example 10

[0055] This embodiment provides an ultrafine denier polyester stretch textured yarn and its preparation method. The specific implementation method is the same as that in Embodiment 1, except that functional filler A is replaced by functional filler H in equal amounts.

[0056] Performance testing The relevant properties of the ultrafine denier polyester stretch textured yarns of Examples 1-10 above were tested, and the test results are shown in Table 1.

[0057] (1) Fracture strength The breaking strength of polyester stretch textured yarn was determined in accordance with the standard GB / T14344-2022 "Test Method for Tensile Properties of Chemical Fiber Filaments". The fiber strength was tested using a single-fiber electronic tensile tester with a pre-tension of 0.5 cN / dtex, a stretching speed of 500 mm / min, and a clamping distance of 500 mm. (2) Antibacterial properties Judging by the antibacterial rate, the antibacterial effect of ultra-fine denier polyester fabric made from ultra-fine denier stretched textured yarn against Escherichia coli and Staphylococcus aureus was used as an example, referring to the national standard GB / T 20944.3-2008.

[0058] Table 1 As shown in Table 1, the ultrafine denier polyester textured yarns in Examples 1-3 of this invention exhibit high breaking strength and show high antibacterial rates against Escherichia coli and Staphylococcus aureus. Examples 4-5 altered the ratio of modified polysiloxane to zinc oxide particles during the preparation of the functional filler, and Examples 6-8 altered the ratio of key substances in the synthesis of modified polysiloxane. Both changes resulted in poor dispersibility and mechanical properties of the prepared functional filler, leading to varying degrees of decrease in the overall breaking strength and antibacterial properties of the polyester fiber. Examples 9 and 10 respectively used commercially available conventional polydimethylsiloxane to replace modified polysiloxane-1 and zinc oxide particles to replace functional filler A in equal amounts. Tests revealed that the ultrafine denier polyester textured yarns exhibited even worse breaking strength and antibacterial properties.

[0059] The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement it. They should not be used to limit the scope of protection of the present invention. All equivalent changes or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A type of ultrafine denier polyester stretch textured yarn, characterized in that, By weight, the ultrafine denier polyester stretch textured yarn comprises the following raw materials: 90-110 parts polyester, 0.6-2 parts functional filler, 1-4 parts lubricant and dispersant, and 1-2 parts low-density polyethylene.

2. The ultrafine denier polyester stretch textured yarn according to claim 1, characterized in that, The polyester is spinning-grade polyethylene terephthalate chips.

3. The ultrafine denier polyester stretch textured yarn according to claim 1, characterized in that, The preparation method of the functional filler includes the following steps: (1) Add potassium hydroxide to an ethanol aqueous solution and stir to obtain a potassium hydroxide solution for later use. Add zinc acetate dihydrate to an ethanol aqueous solution and stir at 75-85℃ for 30-40 min. Cool to room temperature and add potassium hydroxide solution while stirring. Let it age for 30 min, centrifuge, wash, and then add to an ethanol aqueous solution to disperse. Add KH550, stir, centrifuge, wash the precipitate, freeze dry, and obtain zinc oxide particles for later use. (2) Add the modified polysiloxane to tetrahydrofuran, add the zinc oxide particles from step (1), stir, evaporate the solvent, and vacuum dry to obtain the functional filler.

4. The ultrafine denier polyester stretch textured yarn according to claim 3, characterized in that, In step (2), the mass ratio of zinc oxide particles to modified polysiloxane is 1:(1.5-2).

5. The ultrafine denier polyester stretch textured yarn according to claim 3, characterized in that, In step (2), the preparation method of modified polysiloxane includes the following steps: 1) Mix octamethylcyclotetrasiloxane and phenyltris(dimethylsiloxane)silane, add sulfuric acid aqueous solution, stir for 17-18 h, separate the sulfuric acid phase, add sodium bicarbonate, stir, filter, and distill the filtrate under reduced pressure to obtain product 1 for later use. 2) Add product 1 from step 1) into a reaction vessel, pass in an inert gas, add chloroplatinic acid-tetrahydrofuran solution, preheat tert-butyl methacrylate to 75-85℃ and add dropwise, add polymerization inhibitor, react for 8-10 hours, distill under reduced pressure, filter, collect the liquid, and obtain product 2 for later use. 3) Under an inert atmosphere, heat to 85-90℃, add concentrated sulfuric acid to product 2 from step 2), react for 2.5-3.5 hours, cool to room temperature, add to chloroform, wash, separate the chloroform phase, and rotary evaporate to obtain modified polysiloxane.

6. The ultrafine denier polyester stretch textured yarn according to claim 5, characterized in that, In step 1), the mass ratio of octamethylcyclotetrasiloxane to phenyltris(dimethylsiloxane)silane is 1:(0.15-0.4).

7. The ultrafine denier polyester stretch textured yarn according to claim 5, characterized in that, In step 2), the mass ratio of product 1 to tert-butyl methacrylate is 1:(0.4-0.55).

8. The ultrafine denier polyester stretch textured yarn according to claim 1, characterized in that, The lubricating dispersant is polyethylene wax or oxidized polyethylene wax.

9. The ultrafine denier polyester stretch textured yarn according to claim 1, characterized in that, The density of the low-density polyethylene is 0.915-0.925 g / cm³. 3 .

10. A method for preparing ultrafine denier polyester stretch textured yarn according to any one of claims 1-9, characterized in that, Includes the following steps: After melting polyester, functional fillers, lubricating dispersants and low-density polyethylene are added, mixed and extruded to obtain yarn. After cooling, oiling, stretching, and texturing, ultra-fine denier polyester textured yarn is obtained.

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